Accurate measurements of 13C-13C J-couplings in the rhodopsin chromophore by double-quantum solid-state NMR spectroscopy

被引：34

作者：

Lai, WC

McLean, N

Gansmüller, A

Verhoeven, MA

Antonioli, GC

Carravetta, M

Duma, L

Bovee-Geurts, PHM

Johannessen, OG

de Groot, HJM

Lugtenburg, J

Emsley, L

Brown, SP

Brown, RCD

DeGrip, WJ

Levitt, MH ^{[1
]}

机构：

[1] Univ Southampton, Sch Chem, Southampton SO17 1BJ, Hants, England

[2] Leiden Inst Chem, Gorlaeus Labs, NL-2300 RA Leiden, Netherlands

[3] Radboud Univ Nijmegen, Med Ctr, Nijmegen Ctr Mol Life Sci, NL-6500 HB Nijmegen, Netherlands

[4] Univ Warwick, Dept Phys, Coventry CV4 7AL, W Midlands, England

[5] ENS, CNRS, UMR 5182, Lab Chim,Lab Rech Convent,CEA,DSV 23V,DSM 0432, F-69364 Lyon, France

来源：

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY | 2006年 / 128卷 / 12期

基金：

英国生物技术与生命科学研究理事会;

关键词：

D O I：

10.1021/ja0581604

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

A new double-quantum solid-state NMR pulse sequence is presented and used to measure one-bond 13C-13C J-couplings in a set of 13C2-labeled rhodopsin isotopomers. The measured J-couplings reveal a perturbation of the electronic structure at the terminus of the conjugated chain but show no evidence for protein-induced electronic perturbation near the C11-C12 isomerization site. This work establishes NMR methodology for measuring accurate 1JCC values in noncrystalline macromolecules and shows that the measured J-couplings may reveal local electronic perturbations of mechanistic significance. Copyright © 2006 American Chemical Society.

引用

收藏

页码：3878 / 3879

页数：2

相关论文

共 15 条

[1] Determining hydrogen-bond strengths in the solid state by NMR:: the quantitative measurement of homonuclear J couplings [J].

Brown, SP ;

Pérez-Torralba, M ;

Sanz, D ;

Claramunt, RM ;

Emsley, L .

CHEMICAL COMMUNICATIONS, 2002, (17) :1852-1853

[2] Symmetry principles for the design of radiofrequency pulse sequences in the nuclear magnetic resonance of rotating solids [J].

Carravetta, M ;

Edén, M ;

Zhao, X ;

Brinkmann, A ;

Levitt, MH .

CHEMICAL PHYSICS LETTERS, 2000, 321 (3-4) :205-215

[3] Protein-induced bonding perturbation of the rhodopsin chromophore detected by double-quantum solid-state NMR [J].

Carravetta, M ;

Zhao, X ;

Johannessen, OG ;

Lai, WC ;

Verhoeven, MA ;

Bovee-Geurts, PHM ;

Verdegem, PJE ;

Kiihne, S ;

Luthman, H ;

de Groot, HJM ;

deGrip, WJ ;

Lugtenburg, J ;

Levitt, MH .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2004, 126 (12) :3948-3953

[4] 1H and 13C MAS NMR evidence for pronounced ligand-protein interactions involving the ionone ring of the retinylidene chromophore in rhodopsin [J].

Creemers, AFL ;

Kiihne, S ;

Bovee-Geurts, PHM ;

DeGrip, WJ ;

Lugtenburg, J ;

de Groot, HJM .

PROCEEDINGS OF THE NATIONAL ACADEMY OF SCIENCES OF THE UNITED STATES OF AMERICA, 2002, 99 (14) :9101-9106

[5] Transverse dephasing optimized solid-state NMR spectroscopy [J].

De Paëpe, G ;

Giraud, N ;

Lesage, A ;

Hodgkinson, P ;

Böckmann, A ;

Emsley, L .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2003, 125 (46) :13938-13939

[6] The performance of phase modulated heteronuclear dipolar decoupling schemes in fast magic-angle-spinning nuclear magnetic resonance experiments [J].

De Paëpe, G ;

Lesage, A ;

Emsley, L .

JOURNAL OF CHEMICAL PHYSICS, 2003, 119 (09) :4833-4841

[7] Principles of spin-echo modulation by J-couplings in magic-angle-spinning solid-state NMR [J].

Duma, L ;

Lai, WC ;

Carravetta, M ;

Emsley, L ;

Brown, SP ;

Levitt, MH .

CHEMPHYSCHEM, 2004, 5 (06) :815-833

[8] Structure and wavelength modification in retinylidene iminium salts [J].

Elia, GR ;

Childs, RF ;

Britten, JF ;

Yang, DSC ;

Santarsiero, BD .

CANADIAN JOURNAL OF CHEMISTRY-REVUE CANADIENNE DE CHIMIE, 1996, 74 (04) :591-601

[9]

Ernst OP, 2003, COMP SER PHOTOCHEM, V3, P77

[10] An improved broadband decoupling sequence for liquid crystals and solids [J].

Fung, BM ;

Khitrin, AK ;

Ermolaev, K .

JOURNAL OF MAGNETIC RESONANCE, 2000, 142 (01) :97-101